CN114578626A - Electrochromic device and preparation method and application thereof - Google Patents
Electrochromic device and preparation method and application thereof Download PDFInfo
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- CN114578626A CN114578626A CN202210275259.1A CN202210275259A CN114578626A CN 114578626 A CN114578626 A CN 114578626A CN 202210275259 A CN202210275259 A CN 202210275259A CN 114578626 A CN114578626 A CN 114578626A
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/15—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect
- G02F1/1514—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material
- G02F1/1523—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on an electrochromic effect characterised by the electrochromic material, e.g. by the electrodeposited material comprising inorganic material
Abstract
The invention discloses an electrochromic device and a preparation method and application thereof. The electrochromic device comprises a first conducting layer, an electrochromic layer, an electrolyte layer and a second conducting layer which are sequentially stacked, wherein the electrochromic layer is WO doped with carbon nano tubes3And (3) a layer. The preparation method of the electrochromic device comprises the following steps: 1) preparing a tungsten source and a carbon nano tube into a composite dispersion liquid; 2) coating the composite dispersion liquid on the first conductive layer, and drying and annealing to form an electrochromic layer; 3) attaching the second conducting layer to the electrochromic layer, and reserving a perfusion gap of the electrolyte solution; 4) and (4) pouring an electrolyte solution into the reserved gap, and sealing the whole device to obtain the electrochromic device. The electrochromic device has the advantages of high ion diffusion rate, short response time, good electrochromic performance and the like, is simple in preparation process, low in cost, green and energy-saving, and is suitable for large-scale productionAnd (5) practical application.
Description
Technical Field
The invention relates to the technical field of electrochromic devices, in particular to an electrochromic device and a preparation method and application thereof.
Background
Electrochromism refers to a stable and reversible color change phenomenon of optical properties (such as reflectivity, transmittance and absorptivity) of a material under the action of an applied electric field, and the electrochromism shows reversible changes of color and transparency in appearance. The electrochromic device is a practical device formed by packaging an electrochromic material, and the classic structure of the electrochromic device is a sandwich structure formed by laminating an ITO transparent conducting layer (glass plated with the transparent ITO conducting layer), an electrolyte layer, an electrochromic layer and the ITO transparent conducting layer. Electrochromic materials are one of the key factors determining the performance of electrochromic devices, and can be divided into two types according to the materials: 1) inorganic electrochromic material: WO3Etc. as typical representatives; 2) organic electrochromic material: polythiophene and its derivative, viologen, tetrathiafulvalene, metal phthalocyanine compound, etc. The inorganic electrochromic material and the ITO and other inorganic conductive materials have good bonding performance, and the stability of the material obtained by combining the inorganic electrochromic material and the ITO and other inorganic conductive materials is good, so that the inorganic electrochromic material has a huge development prospect. However, the existing electrochromic device using inorganic electrochromic material as electrochromic layer generally has the problems of slow ion diffusion rate, long color conversion time, complex preparation process and the like, and is still difficult to completely meet the requirements of practical application.
Therefore, the development of the electrochromic device with high ion diffusion rate, short response time, good electrochromic performance and simple preparation process is of great significance.
Disclosure of Invention
The invention aims to provide an electrochromic device and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
an electrochromic device comprises a first conductive layer, an electrochromic layer, an electrolyte layer and a second conductive layer which are sequentially stacked; the electrochromic layer is WO doped with carbon nano tubes3And (3) a layer.
Preferably, the conductive material in the first conductive layer is at least one selected from ITO and FTO.
Preferably, the carbon nanotube has a length of 0.4 to 1.3 μm and a diameter of 0.7 to 1.3 nm.
Preferably, the carbon nanotube-doped WO3The thickness of the layer is 200nm to 400 nm.
Preferably, the composition of the electrolyte layer includes an electrolyte and a solvent.
More preferably, the electrolyte layer is formed of an electrolyte solution having a concentration of 0.8mol/L to 1.2 mol/L.
Preferably, the electrolyte is selected from at least one of lithium perchlorate, anhydrous sodium sulfate and potassium sulfate.
Preferably, the solvent is at least one selected from propylene carbonate, ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate.
Preferably, the conductive material in the second conductive layer is selected from at least one of ITO and FTO.
The preparation method of the electrochromic device comprises the following steps:
1) dispersing a tungsten source and a carbon nano tube in a solvent to prepare a composite dispersion liquid;
2) coating the composite dispersion liquid obtained in the step 1) on a first conductive layer, and drying and annealing to form an electrochromic layer;
3) attaching the second conducting layer to the electrochromic layer, and reserving a perfusion gap of the electrolyte solution;
4) and (3) pouring an electrolyte solution into the gap reserved in the step 2), and sealing the whole device to obtain the electrochromic device.
Preferably, the preparation method of the electrochromic device comprises the following steps:
1) mixing the tungsten source dispersion liquid and the carbon nano tube dispersion liquid to prepare a composite dispersion liquid;
2) coating the composite dispersion liquid obtained in the step 1) on the first conducting layer subjected to surface treatment, and drying and annealing to form an electrochromic layer;
3) attaching the second conducting layer subjected to surface treatment to the electrochromic layer, and reserving a perfusion gap of an electrolyte solution;
4) and (3) pouring an electrolyte solution into the gap reserved in the step 2), and sealing the whole device to obtain the electrochromic device.
Preferably, the tungsten source in step 1) is at least one selected from tungsten hexachloride, tungsten powder and sodium tungstate.
Preferably, the mass ratio of the tungsten source to the carbon nanotubes in the composite dispersion liquid in the step 1) is 2000-40000: 1.
Further preferably, the mass ratio of the tungsten source to the carbon nanotubes in the composite dispersion liquid in the step 1) is 3000-14000: 1.
Preferably, the concentration of the tungsten source dispersion liquid in the step 1) is 0.5g/mL to 1.0 g/mL.
Preferably, the concentration of the carbon nanotube dispersion liquid in the step 1) is 0.2mg/mL to 0.5 mg/mL.
Preferably, the volume ratio of the tungsten source dispersion liquid to the carbon nanotube dispersion liquid in the step 1) is 2-8: 1.
Preferably, the drying in the step 2) is carried out at 90-110 ℃, and the drying time is 15-25 min.
Preferably, the annealing in step 2) is specifically performed by: heating to 180-220 ℃ at a heating rate of 40-60 ℃/min, preserving heat for 40-80 s, continuously heating to 270-330 ℃ at a heating rate of 15-25 ℃/min, preserving heat for 60-120 s, and cooling to room temperature at a cooling rate of 8-12 ℃/min.
Preferably, the surface treatment in step 2) is specifically performed by: sequentially carrying out ultrasonic cleaning by using deionized water, absolute ethyl alcohol and isopropanol, drying, and then putting into a UV treatment instrument for ultraviolet irradiation.
Preferably, the coating in step 3) is spin coating.
Preferably, the surface treatment in step 3) is specifically performed by: sequentially carrying out ultrasonic cleaning by using deionized water, absolute ethyl alcohol and isopropanol, drying, and then putting into a UV treatment instrument for ultraviolet irradiation.
Preferably, the sealing in step 4) is made of a UV curable adhesive.
A display device comprises the electrochromic device.
The principle of the invention is as follows: WO (tungsten trioxide) with excellent conductivity and favorable for carbon nanotube doping in electrochromic process3Surface ion implantation and extraction, and electron transport to carbon nanotube and metal oxide WO in the electrochromic layer via the conductive layer when negative bias is applied3Cause H+Insertion of (2), WO3A redox reaction occurs, the color turns blue, and when a positive bias is applied, a cyclical reverse reaction of the above reaction occurs, the equation for the reaction being as follows: WO3+xe-+xH+→HxWO3。
The invention has the beneficial effects that: the electrochromic device has the advantages of high ion diffusion rate, short response time, good electrochromic performance and the like, is simple in preparation process, low in cost, green and energy-saving, and is suitable for large-scale practical application.
Specifically, the method comprises the following steps:
1) the invention adopts the carbon nano tube with excellent conductivity as the enhanced inorganic electrochromic material WO3The carbon nanotube has the advantages of large length-diameter ratio, high specific surface area, large surface energy and the like, and can induce WO3The surface generates a particle cluster structure, which can further lead WO3The prepared electrochromic layer has a rough and porous surface structure, is beneficial to the injection and extraction of ions on the surface of the electrochromic layer, shortens the response time of an electrochromic device, and has electrochromic propertyThe performance is good;
2) the invention adopts the solution method to prepare the electrochromic device, and has the advantages of environmental protection, energy conservation, low cost, simple process and the like.
Drawings
Fig. 1 is a schematic structural view of an electrochromic device of example 1.
The attached drawings indicate the following: 10. a first conductive layer; 20. an electrochromic layer; 30. an electrolyte layer; 40. a second conductive layer.
FIG. 2 is an AFM image of the electrochromic layers formed in examples 1 to 3 and comparative examples 1 to 2.
FIG. 3 is a color change test picture of the electrochromic device of example 1 and comparative examples 1-2 after being energized for 5s in the forward direction.
Fig. 4 is a graph of the transmission spectra of the electrochromic devices of example 1 and comparative example 1.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
an electrochromic device (the structural schematic diagram is shown in fig. 1) comprises a first conductive layer 10, an electrochromic layer 20, an electrolyte layer 30 and a second conductive layer 40 which are sequentially stacked; the electrochromic layer 20 is WO doped with carbon nanotubes3A layer; the first conductive layer 10 and the second conductive layer 40 are both ITO transparent conductive glass sheets, and the ITO transparent conductive glass sheets are composed of glass substrates and ITO conductive layers.
The preparation method of the electrochromic device comprises the following steps:
1) slowly dripping absolute ethyl alcohol into tungsten hexachloride powder, stirring for 4 hours to prepare a tungsten hexachloride absolute ethyl alcohol solution with the concentration of 0.5g/mL, adding carbon nano tubes (the length is 0.4-1.3 mu m, and the diameter is 0.7-1.3 nm) into the absolute ethyl alcohol, performing ultrasonic dispersion to prepare a carbon nano tube absolute ethyl alcohol solution with the concentration of 0.3mg/mL, and mixing the tungsten hexachloride absolute ethyl alcohol solution and the carbon nano tube absolute ethyl alcohol solution according to the volume ratio of 3:1 to prepare a composite dispersion liquid;
2) cutting an ITO transparent conductive substrate (a glass substrate and an ITO conductive layer) into glass sheets with the size specification of 15mm multiplied by 15mm, respectively ultrasonically cleaning the glass sheets with deionized water, absolute ethyl alcohol and isopropanol for 15min, drying, putting the glass sheets into a UV treatment instrument for ultraviolet irradiation for 15min, adsorbing the ITO glass sheets with the surface treated on a turntable of a spin-coating glue spreader (the ITO conductive layer faces upwards), transferring the composite dispersion liquid obtained in the step 1) on the surface of the ITO glass sheets by using a 50 mu L liquid transferring gun, starting the glue spreader to rotationally coat the film, setting the rotational speed of the spin-coating to be 1000rpm before, then transferring to 5000rpm, the time of the spin-coating to be 10s before, then transferring to 40s, then placing the ITO glass sheets with the prepared film on an annealing table, drying the ITO glass sheets for 20min at 100 ℃, heating to 200 ℃ at the heating rate of 50 ℃/min, preserving the temperature for 60s, then continuously heating to 300 ℃ at the heating rate of 20 ℃/min, keeping the temperature for 90s, and then cooling to room temperature at the cooling rate of 10 ℃/min to form an electrochromic layer (the thickness is 330 nm);
3) attaching another ITO glass sheet subjected to surface treatment to the electrochromic layer (the ITO conductive layer faces the electrochromic layer), and reserving a pouring gap of electrolyte solution;
4) LiClO with the concentration of 1mol/L4And (3) filling the propylene carbonate solution into the reserved gap in the step 2) by using a needle cylinder, sealing the whole device by using UV curing adhesive, and curing to obtain the electrochromic device.
Example 2:
an electrochromic device was fabricated in exactly the same manner as in example 1, except that the volume ratio of the tungsten hexachloride absolute ethanol solution and the carbon nanotube absolute ethanol solution in step 1) was adjusted from 3:1 to 8: 1.
Example 3:
an electrochromic device was fabricated in exactly the same manner as in example 1, except that the volume ratio of the tungsten hexachloride absolute ethanol solution and the carbon nanotube absolute ethanol solution in step 1) was adjusted from 3:1 to 2: 1.
Comparative example 1:
an electrochromic device was fabricated in exactly the same manner as in example 1, except that the absolute ethanol solution of carbon nanotubes in step 1) was replaced with an equal volume of absolute ethanol.
Comparative example 2:
an electrochromic device was fabricated in exactly the same manner as in example 1, except that the absolute ethanol solution of tungsten hexachloride in step 1) was replaced with an equal volume of absolute ethanol.
And (3) performance testing:
1) atomic Force Microscope (AFM) images of the electrochromic layers in examples 1-3 and comparative examples 1-2 are shown in FIG. 2 (a-e represent examples 1-3 and comparative examples 1-2, respectively).
As can be seen from fig. 2:
a) the doping concentration of the carbon nanotubes in the electrochromic layer of example 2 is lower than that in example 1, the obtained electrochromic layer has lower roughness, less particle agglomeration and relatively weaker ion injection and extraction capacity;
b) the doping concentration of the carbon nanotubes in the electrochromic layer of the embodiment 3 is higher than that in the embodiment 1, the obtained electrochromic layer has higher roughness, more particle agglomeration and better ion injection and extraction capability;
c) as can be seen from comparative example 1 and comparative example 1: the electrochromic layer of the embodiment 1 has obvious particle agglomeration, the surface is rougher, and the ion injection and extraction efficiency is improved;
d) as can be seen from comparative example 1 and comparative example 2: the electrochromic layer of example 1 was more effective in carbon nanotube doping than comparative example 2 using carbon nanotubes alone as the conductive layer.
2) The color change test pictures of the electrochromic devices of example 1 and comparative examples 1-2 after being energized for 5s in the forward direction are shown in FIG. 3 (a-c represent example 1 and comparative examples 1-2, respectively).
As can be seen from fig. 3: example 1 was significantly deeper in coloration depth after 5 seconds of energization than comparative examples 1 and 2, indicating that example 1 had a faster coloration rate than comparative examples 1 and 2.
3) The transmission spectra of the electrochromic devices of example 1 and comparative example 1 are shown in fig. 4(a and b represent example 1 and comparative example 1, respectively).
As can be seen from fig. 4: example 1 doping of carbon nanotubes makes the fade state curve of the device closer to the initial state curve, because doping of carbon nanotubes enhances the ion injection and extraction capability, fewer ions remain in the film after the fade reaction, the electrochromic redox reaction is more sufficient, the composite electrochromic device is more completely restored from the colored state to the fade state, and the curves of the initial state and the fade state are closer.
4) The electrochromic performance parameters of the electrochromic devices of examples 1 to 3 and comparative examples 1 to 2 are shown in the following table:
TABLE 1 electrochromic Performance parameters of the electrochromic devices of examples 1 to 3 and comparative examples 1 to 2
Note:
tinctorial state transmittance and faded state transmittance: the device is used for testing light transmittance after a periodical constant current is applied through a Chi660e electrochemical workstation;
coloration response time and fading response time: the time required for the amplitude of the change in light transmission to reach 90% when the reading device is switched from the tinted state to the bleached state.
As can be seen from Table 1: since the doping concentration of the carbon nanotubes in example 2 is lower than that in example 1, the roughness of the film in example 2 is lower than that in example 1, the particle agglomeration is less, the ion implantation and extraction capability of the film is relatively weak, and the response time of the film in example 2 is longer than that in example 1, however, the transmittance of the device in a faded state is significantly reduced by doping the carbon nanotubes at an excessively high concentration (example 3), and meanwhile, the carbon nanotube material itself has a color, and the light transmittance of the film is affected by excessively high concentration, so that the light modulation capability of the device is reduced, and the application of the device in production and living is not facilitated.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The utility model provides an electrochromic device, constitutes including first conducting layer, electrochromic layer, electrolyte layer and the second conducting layer that stacks gradually the setting, its characterized in that: the electrochromic layer is WO doped with carbon nano tubes3And (3) a layer.
2. The electrochromic device according to claim 1, characterized in that: the length of the carbon nano tube is 0.4-1.3 mu m, and the diameter is 0.7-1.3 nm.
3. Electrochromic device according to claim 1 or 2, characterized in that: WO doped with the carbon nanotube3The thickness of the layer is 200nm to 400 nm.
4. Electrochromic device according to claim 1 or 2, characterized in that: the conductive material in the first conductive layer is selected from at least one of ITO and FTO; the conductive material in the second conductive layer is selected from at least one of ITO and FTO.
5. Electrochromic device according to claim 1 or 2, characterized in that: the composition of the electrolyte layer comprises an electrolyte and a solvent; the electrolyte is selected from at least one of lithium perchlorate, anhydrous sodium sulfate and potassium sulfate; the solvent is at least one selected from propylene carbonate, ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate.
6. The method for producing an electrochromic device according to any one of claims 1 to 5, characterized by comprising the steps of:
1) dispersing a tungsten source and a carbon nano tube in a solvent to prepare a composite dispersion liquid;
2) coating the composite dispersion liquid obtained in the step 1) on a first conductive layer, and drying and annealing to form an electrochromic layer;
3) attaching the second conducting layer to the electrochromic layer, and reserving a perfusion gap of the electrolyte solution;
4) and (3) pouring an electrolyte solution into the gap reserved in the step 2), and sealing the whole device to obtain the electrochromic device.
7. The method for producing an electrochromic device according to claim 6, characterized in that: the tungsten source in the step 1) is at least one selected from tungsten hexachloride, tungsten powder and sodium tungstate.
8. The method for producing an electrochromic device according to claim 6 or 7, characterized in that: the mass ratio of the tungsten source to the carbon nano tube in the composite dispersion liquid in the step 1) is 2000-40000: 1.
9. The method for producing an electrochromic device according to claim 6 or 7, characterized in that: the drying in the step 2) is carried out at the temperature of 90-110 ℃, and the drying time is 15-25 min; the annealing in the step 2) comprises the following specific operations: heating to 180-220 ℃ at a heating rate of 40-60 ℃/min, preserving heat for 40-80 s, continuously heating to 270-330 ℃ at a heating rate of 15-25 ℃/min, preserving heat for 60-120 s, and cooling to room temperature at a cooling rate of 8-12 ℃/min.
10. A display device comprising the electrochromic device according to any one of claims 1 to 5.
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Cited By (1)
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| CN116203772A (en) * | 2023-02-16 | 2023-06-02 | 安徽精一门科技发展有限公司 | Proton transfer-based quick response electrochromic device and preparation method thereof |
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